第二法(填充柱法)
色譜條件與系統(tǒng)適用性試驗 用直徑為0.18~0.25mm的二乙烯苯-乙基乙烯苯型高分子多孔小球作為載體;柱溫125℃。理論板數(shù)按甲醇峰計算應(yīng)不低于1500;甲醇峰、乙醇峰與內(nèi)標(biāo)物質(zhì)各相鄰色譜峰之間的分離度應(yīng)符合規(guī)定。
校正因子測定 精密量取正丙醇1ml,置100ml量瓶中,用水溶解并稀釋至刻度,搖勻,作為內(nèi)標(biāo)溶液。另精密量取甲醇1ml,置100ml量瓶中,用水稀釋至刻度,搖勻,精密量取10ml,置100ml量瓶中,精密加入內(nèi)標(biāo)溶液10ml,用水稀釋至刻度,搖勻,取1μl注入氣相色譜儀,連續(xù)進(jìn)樣3~5次,測定峰面積,計算校正因子。
測定法 精密量取內(nèi)標(biāo)溶液1ml,置10ml量瓶中,加供試液至刻度,搖勻,作為供試品溶液,取lμl注入氣相色譜儀,測定,即得。
除另有規(guī)定外,供試液含甲醇量不得過0.05% (ml/ml)?。
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編號:20231007007
型號:HQ填充柱
規(guī)格:2m*1/8,60-80目
*高使用溫度:200°C
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Second method (filled column method)
Chromatographic conditions and system suitability tests were carried out using porous microspheres of divinylbenzene ethylenebenzene type polymers with a diameter of 0.18-0.25mm as carriers; The column temperature is 125 ℃. The number of theoretical plates calculated based on methanol peak should not be less than 1500; The resolution between the methanol peak, ethanol peak, and adjacent chromatographic peaks of the internal standard substance should comply with regulations.
Precision measurement of calibration factor: Take 1ml of n-propanol and place it in a 100ml volumetric flask. Dissolve and dilute with water to the mark, shake well, and use it as the internal standard solution. Accurately measure 1ml of methanol and place it in a 100ml volumetric flask. Dilute with water to the mark, shake well. Accurately measure 10ml and place it in a 100ml volumetric flask. Accurately add 10ml of internal standard solution and dilute with water to the mark, shake well, and take 1 μ Inject into the gas chromatograph, continuously inject 3-5 times, measure the peak area, and calculate the correction factor.
Precision measurement method: Take 1ml of the internal standard solution, place it in a 10ml volumetric flask, add the test solution to the mark, shake well, and use it as the test solution. Take l μ Inject into a gas chromatograph, measure, and obtain.
Unless otherwise specified, the methanol content of the test solution shall not exceed 0.05% (ml/ml).
No.: 20231007007
Model: HQ filled column
Specification: 2m * 1/8, 60-80 mesh
*High operating temperature: 200 ° C
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